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Hydrazine hydrate (1:1) → 2,3-Dichloro-4-trifluoromethyl-phenylhydrazine

HRID 2107883
ノート
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反応式

HRID 2107883 の反応式
[Cl:1][C:2]1[C:7]([Cl:8])=[C:6](Cl)[CH:5]=[CH:4][C:3]=1[C:10]([F:13])([F:12])[F:11].O.[NH2:15][NH2:16]>N1C=CC=CC=1>[Cl:8][C:7]1[C:2]([Cl:1])=[C:3]([C:10]([F:13])([F:12])[F:11])[CH:4]=[CH:5][C:6]=1[NH:15][NH2:16]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 24654Hydrazine hydrate (1:1)HCID 133082441,2,3-Trichloro-4-(trifluoromethyl)benzene

生成物 1

HCID 139134182,3-Dichloro-4-trifluoromethyl-phenylhydrazine収率 80%

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

100 g (0.4 mol) of 2,3,4-trichlorobenzotrifluoride are initially introduced, 200 ml of pyridine and subsequently 100 g (2.0 mol) of hydrazine hydrate are added, and the mixture is then heated to the reflux temperature for 12 hours. 90% of the pyridine is then removed by distillation, and the residue remaining is stirred into 250 ml of water. The crystalline product is filtered off with suction, washed with some water and dried. 78 g (80% of theory) of 2,3-dichloro-4-trifluoromethyl-phenylhydrazine of melting point 79° to 80° C. are obtained.

後処理

  1. temperaturethe mixture is then heated to the reflux temperature for 12 hours
  2. custom90% of the pyridine is then removed by distillation
  3. filtrationThe crystalline product is filtered off with suction
  4. washwashed with some water
  5. customdried

出典と根拠

ORDレコード
ord-9c5f362dd5d644d8b11057adfd09559e
出典データセット
uspto-grants-1990_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04936892

反応ノート

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